Citation: ZHANG Fu-Yuan, ZHANG Guang-An, XU Juan, ZHAO Zhuo, XU Liang. Determination of Palladium in Spent Automobile Exhaust Catalysts by Bismuth Fire Assay Preconcentration[J]. Chinese Journal of Analytical Chemistry, ;2020, 48(11): 1590-1596. doi: 10.19756/j.issn.0253-3820.191520 shu

Determination of Palladium in Spent Automobile Exhaust Catalysts by Bismuth Fire Assay Preconcentration

School of Metallurgical Engineering, Anhui University of Technology, Ma'anshan 243032, China

Corresponding author: ZHANG Fu-Yuan, sanzhfy@163.com
Received Date: 26 August 2019
Revised Date: 28 August 2020

Fund Project: This work was supported by the National Natural Science Foundation of China (Nos. U1703130, 51904003) and the Anhui Province Key Laboratory of Metallurgy Engineering & Resources Recycling (No. SKF18-01).

A new method for accurate detection of platium group metals in spent automobile exhaust catalysts samples by inductively coupled plasma spectrometry (ICP-OES) combined with fire assay enrichment through green metal bismuth was established. In this work, the ability of selective slag forming in bismuth fire assay was analyzed, the thermodynamic mechanism from the micro level of bismuth concentrate precious metals was revealed, the order of metal reduced in bismuth fire assay was discussed, and the main factors affecting the results of bismuth fire assay were investigated. The result showed that precious metal oxides were reduced prior to Bi₂O₃, Bi₂O₃ was reduced prior to TeO₂, Cu₂O, As₂O₃, PbO, NiO and other impurities, and Bi₂O₃ had a stronger ability to remove impurities such as Te, Cu, As and Ni. Precious metal elements dissolved in metallic bismuth phase could reduce the free energy of the system more than dissolved in slag phase. Each of the samples or above-mentioned powder were mixed with flux and collectors proportionately, such as 48.00 g of bismuth trioxide, 25.00 g of sodium carbonate anhydrous, 5.5 g of wheat flour, slag silicate degree of 1.1, and 1:1 mass ratio of silicon to boron. The mixture was transferred into fire-clay crucibles and fused at the temperature range from 900℃ to 1080℃ in 20 min, and maintained at 1080℃ for 25 min. The quality of bismuth button was 40 g. The average detection value of palladium was 2852 g/t, the extreme difference was 17 g/t with relative standard deviation of 0.21%. The bismuth fire assay for detection of platinum group metals had higher precision and recovery, and the detection error was less than the error range of national standard.
- Spent automobile exhaust catalysts,
- Bismuth fire assay,
- Detection,
- Platinum group metals,
- Palladium
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